Effect of heat treatment on the surface chemical structure of glass

Oxygen speciation from in situ XPS analysis

Joy Banerjee, Vincent Bojan, Carlo G. Pantano, Seong Kim

Research output: Contribution to journalArticle

6 Citations (Scopus)

Abstract

Compositional changes in unleached and acid-leached soda-lime silicate surfaces were tracked with in-vacuo heating and X-ray Photoelectron Spectroscopy. Surface oxygen speciation was determined using a stoichiometry-based algorithm via elemental composition, instead of the typical O 1s peak-fitting approach. Accurate surface hydroxyl quantification is shown to require dehydration at temperatures near 200°C. On the unleached surface, no change in surface hydroxyl density (~2.5 OH/nm2) is observed in the temperature range of 200°C-500°C after the initial dehydration. However, repolymerization in the network (non-bridging oxygen→bridging oxygen) is observed due to volatilization of sodium. The acid-leached surface undergoes sodium out-diffusion from the bulk at sub-Tg temperatures with laterally resolved inhomogeneity and shows a reduction in the concentration of hydroxyls from 4.5 OH/nm2 (200°C) to 3.2 OH/nm2 (500°C) accompanied by an increase in bridging oxygen. These results suggest that when [OH] > 2.5~3/nm2, vicinal OH undergo dehydroxylation with evolution of water, whereas when [OH] < 2.5/nm2, most OHs are non-interacting and isolated (at temperatures below Tg). Furthermore, at temperatures exceeding 300°C, sodium has enough thermal energy to desorb in vacuum and diffuse from the bulk (depending on the abundance & local structure).

Original languageEnglish (US)
Pages (from-to)644-656
Number of pages13
JournalJournal of the American Ceramic Society
Volume101
Issue number2
DOIs
StatePublished - Feb 1 2018

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X-ray spectroscopy
X ray photoelectron spectroscopy
glass
Heat treatment
Oxygen
Glass
oxygen
Hydroxyl Radical
Sodium
sodium
Dehydration
dehydration
temperature
Temperature
dehydroxylation
Silicates
Acids
acid
stoichiometry
Thermal energy

All Science Journal Classification (ASJC) codes

  • Ceramics and Composites
  • Geology
  • Geochemistry and Petrology
  • Materials Chemistry

Cite this

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title = "Effect of heat treatment on the surface chemical structure of glass: Oxygen speciation from in situ XPS analysis",
abstract = "Compositional changes in unleached and acid-leached soda-lime silicate surfaces were tracked with in-vacuo heating and X-ray Photoelectron Spectroscopy. Surface oxygen speciation was determined using a stoichiometry-based algorithm via elemental composition, instead of the typical O 1s peak-fitting approach. Accurate surface hydroxyl quantification is shown to require dehydration at temperatures near 200°C. On the unleached surface, no change in surface hydroxyl density (~2.5 OH/nm2) is observed in the temperature range of 200°C-500°C after the initial dehydration. However, repolymerization in the network (non-bridging oxygen→bridging oxygen) is observed due to volatilization of sodium. The acid-leached surface undergoes sodium out-diffusion from the bulk at sub-Tg temperatures with laterally resolved inhomogeneity and shows a reduction in the concentration of hydroxyls from 4.5 OH/nm2 (200°C) to 3.2 OH/nm2 (500°C) accompanied by an increase in bridging oxygen. These results suggest that when [OH] > 2.5~3/nm2, vicinal OH undergo dehydroxylation with evolution of water, whereas when [OH] < 2.5/nm2, most OHs are non-interacting and isolated (at temperatures below Tg). Furthermore, at temperatures exceeding 300°C, sodium has enough thermal energy to desorb in vacuum and diffuse from the bulk (depending on the abundance & local structure).",
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Effect of heat treatment on the surface chemical structure of glass : Oxygen speciation from in situ XPS analysis. / Banerjee, Joy; Bojan, Vincent; Pantano, Carlo G.; Kim, Seong.

In: Journal of the American Ceramic Society, Vol. 101, No. 2, 01.02.2018, p. 644-656.

Research output: Contribution to journalArticle

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